氢气还原三氯化砷制备高纯砷的工艺研究

Study on the process of hydrogen reduction of arsenic trichloride to prepare high-purity arsenic

高纯砷的制备方法主要有氯化-还原法、升华蒸馏法、As(OR);热分解法、硫化-还原法等。本文以三氯化砷为原料,采用氢气还原工艺制备高纯砷。考察了氢气用量、反应温度、反应时间和压力等对三氯化砷转化率的影响。结果表明:氢气用量为理论计算量n(H_(2))/n(As)=4,反应压力-0.04 MPa,在830 ℃下停留反应80s,三氯化砷转化率为99.99%。5次稳定性实验结果表明,在最优条件下三氯化砷转换率稳定在99%以上,且高纯砷的纯度均达到7N。

The preparation methods of high-purity arsenic mainly include chlorination-reduction method,sublimation distillation method,As(OR);thermal decomposition method,vulcanization-reduction method,etc.In this paper,high-purity arsenic was prepared by hydrogen reduction process using arsenic trichloride as raw material.The effects of hydrogen dosage,reaction temperature,reaction time and pressure on arsenic trichloride conversion rate were investigated.The results showed that the hydrogen dosage was the theoretically calculated amount n(H_(2))/n(As)=4,the reaction pressure was-0.04 MPa,the reaction was 80s at 830 ℃,and the conversion rate of arsenic trichloride was 99.99%.The results of five stability experiments show that the conversion rate of arsenic trichloride is stable at more than 99% under optimal conditions,and the purity of high-purity arsenic reaches 7N.